WO2016172561A1 - Surfaces rugueuses glissantes - Google Patents

Surfaces rugueuses glissantes Download PDF

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Publication number
WO2016172561A1
WO2016172561A1 PCT/US2016/028959 US2016028959W WO2016172561A1 WO 2016172561 A1 WO2016172561 A1 WO 2016172561A1 US 2016028959 W US2016028959 W US 2016028959W WO 2016172561 A1 WO2016172561 A1 WO 2016172561A1
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Prior art keywords
elements
lubricant
μπι
raised
lubricated
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English (en)
Inventor
Xianming Dai
Birgitt M. BOSCHITSCH
Jing Wang
Tak-Sing WONG
Nan Sun
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Penn State Research Foundation
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Penn State Research Foundation
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Priority to US15/568,639 priority Critical patent/US10434542B2/en
Publication of WO2016172561A1 publication Critical patent/WO2016172561A1/fr
Anticipated expiration legal-status Critical
Priority to US16/551,895 priority patent/US12076748B2/en
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/02—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a matt or rough surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B17/00—Methods preventing fouling
    • B08B17/02—Preventing deposition of fouling or of dust
    • B08B17/06—Preventing deposition of fouling or of dust by giving articles subject to fouling a special shape or arrangement
    • B08B17/065—Preventing deposition of fouling or of dust by giving articles subject to fouling a special shape or arrangement the surface having a microscopic surface pattern to achieve the same effect as a lotus flower
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
    • B29C59/02—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing
    • B29C59/022—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing characterised by the disposition or the configuration, e.g. dimensions, of the embossments or the shaping tools therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
    • B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
    • B32B3/30—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by a layer formed with recesses or projections, e.g. hollows, grooves, protuberances, ribs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
    • B05D3/101—Pretreatment of polymeric substrate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
    • B29C59/02—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing
    • B29C59/022—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing characterised by the disposition or the configuration, e.g. dimensions, of the embossments or the shaping tools therefor
    • B29C2059/023—Microembossing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
    • B29K2995/0037—Other properties
    • B29K2995/0092—Other properties hydrophilic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
    • B29K2995/0037—Other properties
    • B29K2995/0093—Other properties hydrophobic

Definitions

  • the present disclosure relates to substrates having a textured surface and a conformal lubricant layer thereover which can be used for fog harvesting, dropwise condensation, oil adsorption, oil/water separation, drag reduction, anti-fouling and anti-biofouling, anti-frosting and anti-icing devices and applications.
  • Enhancing the mobility of liquid droplets on rough surfaces is of great interest in industry. Applications range from condensation heat transfer to water harvesting to the prevention of icing and frosting.
  • the mobility of a liquid droplet on a rough solid surface has long been associated with its wetting state. When liquid drops are sitting on the tips of solid textures and air is trapped underneath, they are in the Cassie state. When the drops are impregnated within the solid textures, they are in the Wenzel state. The Cassie state has been associated with high droplet mobility, while the Wenzel state has been associated with droplet pinning.
  • Many plants, insects, and animals have highly liquid repellent surfaces, with well- known examples including lotus leaves, the legs of water striders, and the feet of tokay geckos.
  • the liquid repellent function of these natural surfaces is attributed to the presence of hydrophobic hierarchical micro- and nanoscale surface textures that maintain liquid droplets in the Cassie state.
  • Surface textures yielding Cassie state droplets are surfaces with superhydrophobic or superomniphobic properties, with a typical liquid contact angle over 150° and contact angle hysteresis less than 10°. Liquids on these surfaces can roll off with minimal tilting owing to the reduced liquid-solid contact area.
  • a range of engineered superhydrophobic or superomniphobic surfaces have been developed over the last decade with technological applications ranging from self-cleaning surfaces to drag reduction coatings.
  • Liquid droplets on rough surfaces typically exhibit Cassie state, Wenzel state, or a combination of these two states. It is often desirable to maintain high liquid repellency in industrial applications, such as fog harvesting, dropwise condensation, and anti-icing. Because the conventional Wenzel state has long been associated with droplet pinning, intense research has focused on maintaining liquid droplets in the Cassie state. Sustaining a droplet in this state is difficult under certain conditions, however, as the air layer underneath the droplets can be disrupted when subjected to high pressure or high temperature, or when encountering liquids with impurities or low surface tensions. Once the air layer is depleted, the liquid will impregnate the solid textures. As a result, the liquid strongly adheres to the solid surface due to the increased contact area of the liquid-solid interfaces and liquid pinning at defects in the solid substrate.
  • An advantage of the present disclosure is a surface design that can maintain droplet mobility in both the Cassie and Wenzel states.
  • Such slippery rough surfaces advantageously have a high surface area and slippery interface and can be used in fog harvesting, dropwise condensation, oil adsorption, oil/water separation, drag reduction, anti-fouling and anti- biofouling, and anti-icing/frosting devices and applications.
  • a textured surface that can maintain droplet mobility in both the Cassie and Wenzel states.
  • the textured surface can include a plurality of raised first elements and a plurality of second elements thereon and a conformal lubricant layer over the plurality of raised first elements and covering the plurality of second elements.
  • the conformal lubricant layer can have a uniform thickness over the plurality of raised first elements since the thickness is governed by the height of the second elements.
  • the plurality of raised first elements can have an average height of between 0.5 ⁇ and 500 ⁇
  • the plurality of second elements can have an average height of between 0.01 ⁇ and 10 ⁇
  • the substrate can include a silanized coating between the conformal lubricant layer and either the plurality of raised first elements or the plurality of second elements or both.
  • the lubricant can be one or more of an oleophobic lubricant, an oleophilic lubricant, a hydrophobic lubricant and/or a hydrophilic lubricant.
  • Another aspect of the present disclosure includes a method of preparing a slippery rough surface.
  • the method comprises texturing a surface of a substrate with a plurality of raised first elements and a plurality of second elements thereon; and applying a lubricant layer over the plurality of raised first elements and between the plurality of second elements.
  • the lubricant layer can be applied to form a conformal lubricant layer over the plurality of raised first elements.
  • the method can advantageously be applied to surfaces of the substrates that are metals, plastics, ceramics, glass or combinations thereof.
  • the method includes silanizing the textured surface prior to applying the lubricant layer.
  • Figs, la-le illustrate the fabrication of a slippery rough surface and droplets in a Cassie and Wenzel state on such a surface.
  • Figs, la - c show a method including texturing a surface of a substrate with a plurality of raised first elements and a plurality of second elements thereon; silanizing the textured surface; and applying a lubricant layer over the plurality of raised first elements and fully covering the plurality of second elements.
  • the bright area between the droplet and solid surface indicates the existence of a gas layer, e.g., air.
  • the sliding angle is 8°.
  • the drop volumes are 10 and all images share the same scale bar.
  • Figs. 2a-2f are characterizations of surface retention force of water droplets on lubricated and non-lubricated rough surfaces. Note that lubricated rough surface is equivalent to slippery rough surface.
  • Fig. 2a shows an SEM image of a silicon micropillar;
  • Fig. 2b shows an SEM image of a nanotextured micropillar. Nanostructures were formed at the top and side walls of the micropillar and the bottom of the substrate by a wet etching process.
  • Fig. 2c shows an ESEM image of a lubricated micropillar.
  • the lubricant (Krytox 101) was retained within the nanotextures and the lubricated micropillars exhibit flat surface topography similar to that of the silanized micropillar without nanotextures.
  • Fig. 2d is a cross section of bare micropillars
  • Fig. 2f is a chart plotting the retention force F of liquid droplets on lubricated rough surfaces over surface roughness R (R is defined as the ratio of the actual surface area of the elements and the projected area). The coefficient of determination is 0.996 for the linear fit curve depicted here. Error bars indicate standard deviations from three independent measurements.
  • Fig. 3 shows experimentally measured apparent contact angles of various liquid droplets in the Wenzel state as a function of surface roughness of the slippery rough surfaces. It illustrates the wetting characteristics of the slippery rough surfaces.
  • Experimental data includes the apparent static, advancing, and receding angles of different liquids. Error bars represent the standard deviation of at least three data points. Because slippery rough surfaces allow for Wenzel state droplet mobility, and thus lower contact angle hysteresis compared to conventional Wenzel state droplets, we can measure the apparent contact angle with higher accuracy. More accurate experimental measurements allow for more accurate verification of equations predicting apparent contact angle.
  • Figs. 4a-4e show aqueous and organic liquid droplets in the Wenzel state on lubricated and non-lubricated rough surfaces. Note that lubricated rough surface is equivalent to slippery rough surface.
  • Fig. 4a is schematic of a drop with low surface tension in Wenzel state on a lubricated rough surface, showing a low contact angle.
  • Fig. 4b shows a 10 ⁇ L droplet of hexadecane on the lubricated rough surfaces, displaying a sliding angle of 15°.
  • Fig. 4c is a schematic of a drop with low surface tension on silanized micropillars, showing a low contact angle in Wenzel state.
  • Fig. 4a-4e show aqueous and organic liquid droplets in the Wenzel state on lubricated and non-lubricated rough surfaces. Note that lubricated rough surface is equivalent to slippery rough surface.
  • Fig. 4a is schematic of a drop with low surface tension in Wenzel state on a
  • FIG. 4d shows a 10 droplet of hexadecane on microstructured surfaces with a tilt angle of 90°. The drop is strongly pinned on the surface, exhibiting the sticky Wenzel state.
  • Figs. 4b and 4d share the same scale bar. Error bars indicate standard deviations from three independent measurements.
  • Fig. 5 is a plot showing fog harvesting performance of superhydrophobic surface (SHS), slippery liquid-infused porous surface (SLIPS) and slippery rough surface (SRS).
  • SHS superhydrophobic surface
  • SLIPS slippery liquid-infused porous surface
  • SRS slippery rough surface
  • Figs. 6a-6d show the characterization of nanotextured micropillars.
  • Fig. 6a shows patterned nanotextured micropillars;
  • Fig. 6b shows nanotextures on top and side walls of a micropillar;
  • Fig. 6c is a top view of the nanotextures;
  • Fig. 6d is a cross section of nanotextured micropillars.
  • Figs. 7a-7d shows the lubrication results of a textured surface having a plurality of raised elements in the form of micropillars.
  • Fig. 7a is a cross section of the lubricated micropillars. The nanotextures were submerged in lubricants.
  • Figs. 7b, c, d show ESEM image of the lubricant distribution: spin speed 3000, 5000 and 12000 rpm. The spin time is 60 seconds. Notice that at spin speeds higher than 8000 rpm, the lubricant uniformly covers the nanotextures, yielding a slippery rough surface. Depending on the viscosity of the lubricant, the spin speed and speed duration will be adjusted accordingly.
  • Figs. 8a-8f show the contact angles of water droplets on Krytox 101 lubricated microstructures.
  • Fig. 8a has a Krytox 101 infused nanotextured plain surface.
  • Fig. 9 is a chart showing the retention forces of water droplets on the lubricated rough surfaces with different pillar heights. Error bars represent the standard deviation for three independent measurements.
  • Figs. 10a- 10b are charts showing the wrapping layer effect on the liquid repellency of slippery rough surfaces Fig. 10a shows lubrication with Krytox 101 and Fig. 10b shows lubrication with mineral oil. Error bars represent the measurement error for a single water droplet.
  • Figs. 11 a- l ib show contact angles for various lubricants.
  • Fig. 11a plots contact angle hysteresis of water droplet on various lubricants; and
  • Fig. l ib plots experimental contact angle and the prediction of modified Young's equation.
  • Fig. 12 is a plot showing the comparison of liquid repellency performances between slippery rough surfaces (in both Cassie and Wenzel state) and superhydrophobic surfaces after the surfaces have been submerged into the bacterial solutions at specific period of time. Note that the dotted line indicated that the water droplets wet and pin onto the superhydrophobic surface.
  • the present disclosure relates to a substrate having a textured surface that can maintain and/or advance droplet mobility in both the Cassie and Wenzel states, e.g., a slippery rough surface (SRS).
  • the textured surface includes a plurality of raised first elements and a plurality of second elements thereon and a conformal lubricant layer over the plurality of raised first elements and covering the plurality of second elements, e.g. between and fully covering the plurality of second elements.
  • the plurality of raised first elements have an average height of between 0.5 ⁇ and 500 ⁇ , e.g., an average height of between 15 ⁇ and 100 ⁇
  • the plurality of second elements have an average height of between 0.01 ⁇ and 10 ⁇ , e.g., an average height of between 0.5 ⁇ and 5 ⁇ .
  • the surface roughness R is between 1 and 1.4 in FIG 2f.
  • the substrate can further comprise a silanized coating between the conformal lubricant layer and either the plurality of raised first elements or the plurality of second elements or both.
  • silanization means to contact the surface of the substrate with at least one reactive silane to chemically react the surface of the substrate and thus bind the silane to the substrate surface.
  • a silanized coating results from such silanization.
  • Reactive silanes that can be used for silanization are known in the art and include, for example, heptadecafluoro- 1 , 1 ,2,2- tetrahydrodecyltrichlorosilane, trimethylchlorosilane, perfluorinated silanes, etc.
  • the textured surface includes a plurality of raised elements and a conformal lubricant layer over the plurality of raised elements, wherein the conformal lubricant layer has a uniform thickness over the plurality of raised elements, which have random or regular distributions.
  • the conformal lubricant layer forms an energetically stable and atomically smooth lubricant layer.
  • the plurality of raised first elements have an average height of between 0.5 ⁇ and 500 ⁇ . The height is determined from the bottom and top of a single structure.
  • the conformal lubricant layer can be one or more of an oleophobic lubricant, an oleophilic lubricant, a hydrophobic lubricant and/or a hydrophilic lubricant.
  • the conformal lubricant layer can be tertiary perfluoroalkylamines (such as perfluorotri- npentylamine, FC-70 by 3M; perfluorotri-n-butylamine FC-40, etc.), perfluoroalkylsulfides and perfluoroalkylsulfoxides, perfluoroalkylethers, perfluorocycloethers (like FC-77) and perfluoropolyethers (such as KRYTOX family of lubricants by DuPont), perfluoroalkylphosphines, perfluoroalkylphosphineoxides and their mixtures can be used for these applications, as well as their mixtures with perfluor
  • the thickness of the lubricant layer is preferably between 0.01 ⁇ and 10 ⁇ , which is close to the height of the nanotextures in certain embodiments.
  • the uniformity of the lubricant layer over the raised plurality of elements is preferably less than 10 ⁇ .
  • the lubricant and silanization agent can be matched to a given substrate.
  • perfluorinated oils and perfluorinated silanes can be a combination on the substrate.
  • Hydrophobic combination include, for example, mineral oils, hydrocarbons, and trimethylchlorosilane and hydrophilic combinations include, for example, hydroxyl PDMS and trimethylchlorosilane.
  • Substrates and textured surfaces that can be used in the present disclosure include those of silicon, metals (e.g., copper, aluminum, steel, titanium etc. and their alloys, e.g., stainless steel, etc.), ceramics (e.g., glass), and polymers or other materials.
  • substrates having a textured surface can be used in a variety of devices.
  • the substrates having a textured surface of the present disclosure can be used in evaporators, condensers, heat exchangers, water and oil collector devices, and drag reduction and anti-biofouling coatings.
  • the slippery rough surfaces in the present disclosure mimic an idealized rough surface.
  • impregnated liquid droplets can show high droplet mobility on hierarchically micro- and nano-textured surfaces in which the nanostructures alone are infused with lubricant (Fig. lc).
  • Fig. lc we show that by infusing a microscopically-thin conformal layer of lubricant on the surface nanotextures, the sharp edges can be smoothened by the liquid lubricant and the pinning effect can be greatly reduced, leading to enhanced droplet mobility in both Wenzel and Cassie states (Figs. Id, le).
  • a slippery rough surface can be prepared by texturing a surface of a substrate with a plurality of raised first elements and a plurality of second elements thereon; and applying a lubricant layer over the plurality of raised first elements and fully covering the plurality of second elements.
  • the lubricant can be applied to form a conformal lubricant layer over the plurality of raised first elements and preferably with a uniform thickness.
  • the thickness of the conformal lubricant layer is between 0.01 ⁇ and 10 ⁇ .
  • it is preferable that the thickness does not vary over the plurality of raised elements by more than 100%.
  • the rough surfaces should allow the lubricant to stably wet and conformally adhere to the solid textures.
  • it should be energetically more favorable for the lubricant, rather than foreign liquids, to wet the solid textures.
  • the lubricant and foreign liquids should be immiscible.
  • the first criterion can be satisfied by creating nanoscale textures on micropillars, thus forming hierarchical structures, i.e., a plurality of raised first elements and a plurality of second elements thereon.
  • R the roughness resulting from the micropillars alone
  • r the roughness resulting from nanotextures on the micropillars.
  • the second criterion can be satisfied by choosing an appropriate solid and lubricant combination for an immiscible foreign fluid such that the following relationships are satisfied:
  • perfluorinated silanes to functionalize the silicon hierarchical textures and perfluorinated lubricants (i.e., DuPontTM Krytox oils) for the lubrication.
  • perfluorinated lubricants are known to be immiscible to both the aqueous and oil phases, and are hydrophobic in nature.
  • the measured intrinsic contact angle, ⁇ , of water droplets on a smooth slippery surface lubricated with perfluorinated lubricant is 121.1° ⁇ 1.0°.
  • the height of the silicon nanotextures is 5.1 ⁇ on the top of the micropillars, and 3.8 ⁇ on the side wall.
  • the roughness of the nanotextures, r was estimated to be 14.6 ⁇ 0.3 on the side of the micropillar and 19.3 ⁇ 0.4 on the top of the micropillar through image analysis of high resolution scanning electron micrographs.
  • the lubricant was applied onto the solid substrate by a spin-coating process, where excess lubricant was removed from the micropillar structures at high spin speed. Due to the dominance of capillary force per unit volume at smaller length scales, the nanotextures will help retain the lubricant more favorably compared to the microscopic roughness.
  • the strong chemical affinity of the silane coatings to the perfluorinated lubricant together with the high roughness of the nanotextures allowed the lubricant to completely infuse the nanotextures and formed a conformal layer over the micropillar structures (see Figs. 2b and 2c).
  • the surface morphology of the micropillars was smooth with round edges as confirmed by high-resolution electron microscope.
  • the non- lubricated and lubricated micropillars have similar surface morphology based on the cross sectional images (Figs. 2d and 2e) and ESEM images (Fig. 2c).
  • F the retention force of the Wenzel state droplet on lubricated micropillars normalized by that on non-lubricated ones with the same surface roughness.
  • F * ranges from -10% for high surface tension (72.4 mN/m) fluids to -36% for low surface tension fluids (19.9 mN/m).
  • the measured retention force values of Wenzel drops on these lubricated surfaces are significantly lower than those on non-lubricated surfaces (Fig. 4e). This is attributed to the reduction of pinning through smoothening of micro/nanoscopic edges by the lubricant. These results demonstrate that lubricated rough surfaces can substantially reduce retention force and thus enhance drop mobility of Wenzel drops with various surface tensions.
  • the slippery rough surface (of depth -20 ⁇ ) exhibited a fog harvesting rate of 376.0 mg/(hrcm ) (mg - milligram, hr - hour, cm - centimeter), which is 22.2% faster than SLIPS and 136.8% faster than SHS (Fig. 5).
  • the slippery rough surface exhibited enhanced drop nucleation and coalescence, resulting in faster droplet removal.
  • microscopic liquid droplets were pinned onto the surface structures due to large Laplace pressure of the small droplets.
  • SHS displayed a much smaller droplet removal rate compared to that of slippery rough surfaces.
  • the fog harvesting rate on slippery rough surfaces increased by 11.1% (Fig. 5). This indicates that fog harvesting performance can be further optimized by engineering the dimensions of surface structures.
  • the mineral oil was absorbed on the mesh screen due to the superoleophilic nature of the lubricated mesh. Then we quickly take off the mesh screen from the mixture. The absorbed oil dripped off from the mesh completely due to the presence of the slippery interface, demonstrating to its anti-fouling property. Therefore, the lubricated mesh can be recycled without or with minimal cleaning requirement. Additionally, the mesh can collect oil in oil-water emulsion without any fouling.
  • composition of the coatings e.g., viscosity or phase change temperatures of lubricants
  • the longevity of the lubricated rough surfaces can be engineered by choosing lubricants with low evaporation rate, low miscibility, and reduced wrapping of the lubricant around the contacting fluid.
  • the longevity of the lubricants could be further enhanced by infusing these lubricants into polymeric coatings as reservoirs.
  • slippery rough surfaces combine the unique advantages of superhydrophobic surfaces (i.e., high surface area) and SLIPS (i.e., slippery interface) and can repel liquids in any wetting state, these surfaces will find important industrial applications related to liquid harvesting, liquid absorption/separation, and phase change applications.
  • the slippery rough surfaces could further enhance condensation heat transfer as compared to superhydrophobic surfaces, even in relatively high temperature environments such as those that exist in heat exchangers or organic Rankine cycles. In icing condition, the lubricated rough surfaces could readily shed off liquid condensates in the Wenzel state to delay frost and ice formation.
  • lubricated rough surfaces could provide water harvesting in high humidity conditions faster than the state-of-the art liquid-repellent surfaces. Many of these water condensates have traditionally pinned to the surface texture— a result of irreversible transition from the Cassie state to the "sticky" Wenzel state.
  • the lubricated rough surfaces can also serve as drag reduction and anti-biofouling coatings. The ability to repel fluids in any wetting state may open up new opportunities for scientific studies and engineering applications related to adhesion, nucleation, transport phenomena, and beyond.
  • the wafer was immediately immersed into a solution of 4.8 M HF and 0.01 M silver nitride (AgN0 3 ) for 1 min to deposit catalysts.
  • the Ag + was reduced to Ag nanoparticles, which could be deposited on the top, bottom and side walls of the microstructured silicon surfaces. These Ag nanoparticles acted as catalysts to enhance local etching speed during the etching process.
  • the microstructured wafer with the catalyst was put in the etching solution containing 4.8 M HF and 0.3 M hydrogen peroxide (H 2 O 2 ) for 6 to 7 min. After the catalyst deposition and etching step, the wafer was placed into the dilute nitric acid solution to dissolve the silver dendrites.
  • the wafer was washed with DI water and dried with nitrogen gas. Patterned nanotextured micropillars were obtained on the silicon wafer (Fig. 6a, b and c).
  • the height of the nanotextures is 5.1 ⁇ on the top of the micropillars and 3.8 ⁇ on the side wall, respectively (Fig. 6d).
  • the roughness of the nanotextures was estimated to be 14.6 ⁇ 0.3 on the side of the micropillar and 19.3 ⁇ 0.4 on the top of the micropillar through image analysis of high resolution scanning electron micrographs. Image analyses were conducted using MATLAB.
  • the greyscale image (i.e., an image with pixel intensities ranging over a spectrum from 0 to 1 , where 0 is black and 1 is white) shown in Figure 10c was converted to a binary image (i.e., where pixel intensities are either 0 or 1) based on a set intensity threshold.
  • a binary image i.e., where pixel intensities are either 0 or 1
  • a plateau in the roughness versus threshold value occurred approximately between a threshold of 0.2 and 0.4, so the average of roughness values between these points was used as the roughness.
  • this average roughness was calculated for varying resolutions until convergence was apparent, and a resolution of 40 points proved to be sufficient.
  • Nano-textured aluminum meshes were fabricated by two-step etching processes.
  • the aluminum mesh was washed by diluted hydrochloric acid for 10 min to remove the oxidized layer on the surface.
  • steam was used to oxidize the mesh for 1 hour in atmospheric pressure (101 kPa) to form boehmite nanotextures.
  • the mesh wire is uniformly etched with nanotextures, which is helpful to enhance the hydrophobicity and the lubricant retention on the surface.
  • the diameter of the mesh wire varies from 53 ⁇ to 400 ⁇ .
  • the nano boehmite structure on the wire has a depth of tens of nano meters.
  • the nanotextured silicon microstructures/aluminum mesh were silanized using either heptadecafluoro- 1, 1,2,2- tetrahydrodecyltrichlorosilane (Gelest Inc.) or trimethylchlorosilane (Sigma- Aldrich). These silanes were deposited onto the silicon surfaces in a vacuum chamber for 4 hours, and were deposited onto aluminum mesh in ethanol solution for 20 hours, or less time with higher temperature Afterwards, lubricant such as Krytox 101 (DuPont, viscosity of 17.4 cSt at 20 °C) was coated on the silanized nanotextured micropillars using a spin coater.
  • Krytox 101 DuPont, viscosity of 17.4 cSt at 20 °C
  • the lubricant thickness was controlled by the spin speed of the spin coater. Higher spin speed can remove more lubricants and yield a lubricant layer that is more conformal to the micropillars.
  • the cross sections of micropillars were visualized by a goniometer. Increased spin speed helps to remove the lubricants between two micropillars as shown in the ESEM images of Fig. 7a.
  • Siliconized silicon- 1 refers to nanotextured microstructures were silanized by the heptadecafluoro- 1 , 1 ,2,2- tetrahydrodecyltrichlorosilane and "Silanized silicon-2” refers to those silanized by trimethylchlorosilane.
  • Y indicates that Liquid B can form stable conformally lubricated microstructures.
  • ⁇ A and ⁇ ⁇ represent the surface tensions of Liquid A and Liquid B, respectively (Table 2).
  • ⁇ AB represents the interfacial tension between Liquid A and Liquid B (Table S3).
  • ⁇ and ⁇ are the static contact angles on silanized flat silicon substrate (Table 4).
  • the nanotextures were fully submerged under the lubricant layer.
  • the lubricated micropillars were visualized by an ESEM to capture the distribution of oil lubricants on an angled stage (40° ⁇ 60°).
  • the applied voltage was 20 kV and current was 2.1 nA for the operation of ESEM.
  • the temperature was reduced to -5 °C before the low vacuum was applied.
  • the pressure was set at 3.8 torr, which is much higher than the saturation pressure of Krytox 101 at -5 °C. From the ESEM images (Figs.
  • the surface roughness was calculated based on w, L, and h (See definitions in the main text). Since the lubricant covered the bottom corners of the micropillars, the lubricated micropillars do not have a well-defined geometry (Fig. 7b). We measured h from the top of the lubricated micropillar to the bottom of the lubricated surfaces. When the spin speed is 12000 rpm (Fig. 7d), the calculated roughness closely resembles the actual roughness as verified by the high-resolution electron micrographs.
  • the sliding angle was measured by an automated goniometer (rame-hart) at room temperature (21 - 24 °C) with -20% relative humidity. The system was calibrated each time before the measurements were conducted. The image of the droplet was captured through a camera equipped with the optical system and the drop imaging software measured the contact angle, contact angle hysteresis, and the sliding angle.
  • the stage was tilted automatically at the speed of 1 degree/second and the drop image was captured every second.
  • the sliding angle can be obtained by analyzing those images.
  • the contact line starts to move, the associated tilted angle is taken as the sliding angle.
  • the accuracy of the measurement is ⁇ 0.5°.
  • the measured sliding angles were used to estimate the droplet retention forces on the lubricated rough surfaces with different pillar heights (Fig. 9).
  • Microgrooves on aluminum surface were fabricated using a standard micromachining.
  • the groove size and space between grooves are -200 ⁇ .
  • the aluminum residues and other surface contaminations (e.g., oils) generated from the machining were removed by ultrasonic cleaning in acetone for 15 min.
  • An acid wash process was used to remove an oxidized aluminum layer on the surface, which may inhibit the growth of boehmite nanotexture.
  • the microgrooved aluminum was washed in diluted hydrochloric acid (1 wt. %) for 10 min, and then cleaned by DI water.
  • a water steam etching was used to create boehmite nanotextures on the surfaces of grooves.
  • the microgrooved aluminum cylinder was put in a water steam environment at 100 C° with a pressure of 105 kPa for 20 min.
  • the nanotextured microgrooves were created on aluminum cylinder.
  • Oxygen plasma was conducted before silanization.
  • the nanotextured microgrooved aluminum cylinder was cleaned and surface activated in an oxygen plasma cleaner (Harrick) for 15 min.
  • the nanotextured aluminum microstructures were silanized using 1H, 1H,2H,2H- perfluorodecyltriethoxysilane (Sigma-Aldrich).
  • the silane molecules were deposited onto aluminum in ethanol solution at 80 C° for 4 hours.
  • lubricant such as Krytox 101 (DuPont, viscosity of 17.4 cSt at 20 °C) was coated on the silanized nanotextured microgrooves by spray coating, and excess lubricant between the grooves was removed by a nitrogen gun.
  • the slippery rough surfaces have a wide range of applications, such as water harvesting, dropwise condensation, advanced heat exchange, and refrigeration.
  • Three surfaces, including SHS (i.e., silanized hierarchical microchannels), SLIPS (i.e., lubricant infused nanotextures) and slippery rough surfaces (i.e., microchannels with conformal lubrication) were used to compare their performance in the applications of fog harvesting and dropwise condensation.
  • the micro/nano hierarchical microchannels were fabricated using aforementioned DRIE and wet etching methods.
  • a conventional ultrasonic humidifier (Crane EE-5301) was used to produce cool mist.
  • the lubricated rough substrates were placed vertically, facing the mist. The distance between the outlet of the humidifier and the vertical substrate was -15 cm.
  • the dripping water was collected by a clean beaker.
  • the weight of the beaker before and after collection was measured as 3 ⁇ 4 and M a , respectively.
  • the weight of the lubricated sample before and after collection was measured as M s b and M sa , respectively.
  • the longevity of the lubricated rough surfaces is highly reliant on three factors, including: I) the miscibility of lubricant and the contacting fluid, II) the evaporation rate of the lubricant, as well as III) the wrapping of the lubricant around the contacting fluid.
  • the lubricant should be chosen for its low miscibility, low evaporation rate and reduced wrapping around the contacting fluid. There are many commercial lubricants with negligible solubility with water.
  • solubilities of water in perfluorinated oils, mineral oils, and liquid polydimethylsiloxane are 1.76 mol/m J , 2.14 mol/m 3 and 36 mol/m 3 , respectively 36 .
  • a third factor impacting the longevity of the slippery rough surfaces is the lubricant wrapping layer around the contacting fluid droplet.
  • Such information is important because the formation of a wrapping layer implies the loss of lubricant volume as the droplet slides off of the lubricated surface. This lubricant loss leads to an undesirable decrease in the liquid repellency of the surface.
  • the surface energy of the substrate-lubricant-droplet system is minimized.
  • ⁇ v is the surface tension of the contacting fluid droplet in vapor and Yi ⁇ 2 is the interfacial tension between the contacting fluid droplet and lubricant.
  • a ⁇ is the area of the droplet-vapor interface and A 2 is the area of the droplet-lubricant interface.
  • E 2 Y v (1 - ⁇ ) ⁇ + Y v ⁇ ⁇ + Y ( ⁇ + A 2 ) (Eq. S4) [0101] where ⁇ is the fraction of A ⁇ coated with a lubricant wrapping layer and Y izV is the surface tension of the lubricant in vapor.
  • ⁇ is the fraction of A ⁇ coated with a lubricant wrapping layer
  • Y izV is the surface tension of the lubricant in vapor.
  • the former system must be energetically more favorable than the latter.
  • the criterion for the nonexistence of a full wrapping layer is:
  • Anti-biofouling surfaces are of interest in various fields from medicine to seafaring ship design. In medicine, anti-fouling surfaces would prolong the lifetime of medical devices such as catheters and reduce the spread of disease via surface contamination. In naval applications, such surfaces would prevent barnacle buildup on ships and thus reduce drag and wasted energy. While conventional superhydrophobic surfaces can successfully prevent bio- fouling for short periods of time (i.e., a few hours), organisms such as bacteria can still adhere to the solid surface eventually eliminating its anti-fouling capabilities. Other methods for anti- fouling coatings are to incorporate chemicals such as copper and/or co-biocides to prevent fouling. These options are less than ideal, however, as they either contribute to the rise of "super- bugs" or may pose environmental hazards.
  • Slippery rough surfaces address anti-fouling through a different mechanism— a mechanism similar to that of slippery liquid-infused porous surfaces (SLIPS).
  • SLIPS slippery liquid-infused porous surfaces
  • the conformal liquid layer inhibits bio-fouling because there is no solid surface onto which organisms (such as bacteria) can attach. If they do settle onto the lubricant layer of the SRS, they can be easily removed via shear force as the lubricant layer is mobile.
  • Slippery rough surface can reduce friction and save energy for marine ships.
  • slip length is a measure of drag reduction capability of the surface to a specific test liquid and is independent of dimensions of the flow field.
  • the torque, M is related to the slip length, b, by the following equation derived from the Navier-Stoke equation using Navier's assumption that slip velocity is proportional to the shear rate at the wall,
  • ⁇ fluid viscosity
  • R the cone radius
  • ⁇ the angular velocity of the cone
  • ⁇ the cone angle

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Laminated Bodies (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Lubricants (AREA)

Abstract

La présente invention concerne des substrats présentant une surface texturée qui peut conserver ou améliorer la mobilité des gouttelettes à la fois dans les états de Cassie et Wenzel qui incluent une surface texturée et par dessus une couche de lubrifiant de conformation. La surface texturée peut inclure une pluralité de premiers éléments élevés et une pluralité de seconds éléments dessus et la couche de lubrifiant de conformation par dessus la pluralité des premiers éléments élevés et le recouvrement de la pluralité des seconds éléments. La pluralité des premiers éléments élevés peut présenter une hauteur moyenne comprise entre 0,5 μm et 500 μm, et la pluralité des seconds éléments peut présenter une hauteur moyenne comprise entre 0,01 μm et 10 μm. De tels substrats peuvent être préparés par texturation d'une surface d'un substrat avec une pluralité de premiers éléments élevés et une pluralité de seconds éléments dessus ; la silanisation facultative de la surface texturée et l'application d'une couche de lubrifiant sur la pluralité des premiers éléments élevés et entre la pluralité des seconds éléments.
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